# Copyright The Royal Society of Chemistry, 1999
# CCDC Number: 186/1318
# CIF belonging to Paper -2-Hydroxy-benzylidene .. - Ligtenbarg et al.
# CIF-file generated for s1720a
#==============================================================================
data_global
#==============================================================================
# 0. AUDIT DETAILS
_audit_creation_date 'Wed Sep 23 15:53:22 1998'
_audit_creation_method 'PLATON
option'
#===============================================================================
# 1. SUBMISSION DETAILS
_publ_contact_author_name # Name of author for correspondence
; Dr. A.L. Spek
;
_publ_contact_author_address # Address of author for correspondence
;
Bijvoet Center for Biomolecular Research
Department of Crystal and Structural Chemistry
Utrecht University
Padualaan 8
3584 CH Utrecht
The Netherlands
;
_publ_contact_author_email 'spea@chem.uu.nl'
_publ_contact_author_fax '+31 30 2533940'
_publ_contact_author_phone '+31 30 2532538'
#===============================================================================
data_s1720a
#===============================================================================
# 5. CHEMICAL DATA
_chemical_formula_moiety 'C18 H12 N3 O3 V'
_chemical_formula_sum 'C18 H12 N3 O3 V'
_chemical_formula_weight 369.25
_chemical_compound_source 'see text'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
V V 0.3005 0.5294
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
#===============================================================================
# 6. CRYSTAL DATA
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 21/c'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,1/2+y,1/2-z
-x,-y,-z
x,1/2-y,1/2+z
_cell_length_a 7.0787(16)
_cell_length_b 16.833(5)
_cell_length_c 13.573(5)
_cell_angle_alpha 90
_cell_angle_beta 115.21(2)
_cell_angle_gamma 90
_cell_volume 1463.3(8)
_cell_formula_units_Z 4
_cell_measurement_temperature 150
_exptl_crystal_description block
_exptl_crystal_colour yellow
_exptl_crystal_size_max 0.43
_exptl_crystal_size_mid 0.12
_exptl_crystal_size_min 0.10
_exptl_crystal_density_diffrn 1.676
_exptl_crystal_density_method 'Not Measured'
_exptl_crystal_F_000 752
_exptl_absorpt_coefficient_mu 0.70
_exptl_absorpt_correction_type delref
_exptl_absorpt_process_details PLATON/DELABS
_exptl_absorpt_correction_T_min 0.143
_exptl_absorpt_correction_T_max 0.615
#===============================================================================
# 7. EXPERIMENTAL DATA
_exptl_special_details
; ?
;
_diffrn_ambient_temperature 150
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_source 'Rotating Anode'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'CAD4T'
_diffrn_measurement_method 'omega-scan'
# number of measured reflections (redundant set)
_diffrn_reflns_number 6346
_diffrn_reflns_av_R_equivalents 0.1061
_diffrn_reflns_av_sigmaI/netI 0.1155
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_h_max 0
_diffrn_reflns_limit_k_min -21
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_theta_min 2.05
_diffrn_reflns_theta_max 26.50
# number of unique reflections
_reflns_number_total 3006
# number of observed reflections (> n sig(I))
_reflns_number_gt 1984
_reflns_threshold_expression 'I>2sigma(i)'
_computing_data_collection 'Locally modified CAD4-Version 5 Software'
_computing_cell_refinement 'SET4 (de Boer & Duisenberg, 1984)'
_computing_data_reduction 'HELENA (Spek, 1997)'
_computing_structure_solution 'SHELXS86'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material 'PLATON (Spek, 1990)'
#===============================================================================
# 8. REFINEMENT DATA
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme 'calc'
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0561P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_hydrogen_treatment 'H-atom refinement: see text '
_refine_ls_extinction_method none
_refine_ls_abs_structure_details none
_refine_ls_abs_structure_Flack none
_refine_ls_number_reflns 3006
_refine_ls_number_parameters 226
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0992
_refine_ls_R_factor_gt 0.0579
_refine_ls_wR_factor_ref 0.1415
_refine_ls_wR_factor_gt 0.1237
_refine_ls_goodness_of_fit_ref 1.017
_refine_ls_restrained_S_all 1.017
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 0.592
_refine_diff_density_min -0.547
_refine_diff_density_rms 0.089
#===============================================================================
# 9. ATOMIC COORDINATES AND THERMAL PARAMETERS
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
V1 V Uani 0.48998(12) 0.57903(4) 0.30698(5) 1.000 0.0219(2)
O1 O Uani 0.3133(5) 0.52189(16) 0.1818(2) 1.000 0.0253(8)
O2 O Uani 0.6349(5) 0.63471(18) 0.2711(2) 1.000 0.0279(9)
O3 O Uani 0.3167(5) 0.63423(16) 0.3241(2) 1.000 0.0262(9)
N1 N Uani 0.6258(5) 0.46685(18) 0.3526(2) 1.000 0.0198(9)
N2 N Uani 0.7201(5) 0.34208(18) 0.3607(2) 1.000 0.0184(9)
N3 N Uani 0.6724(6) 0.58101(19) 0.4825(2) 1.000 0.0238(10)
C1 C Uani 0.3605(7) 0.4666(2) 0.1253(3) 1.000 0.0217(11)
C2 C Uani 0.2540(7) 0.4697(3) 0.0107(3) 1.000 0.0272(12)
C3 C Uani 0.2977(7) 0.4159(3) -0.0526(3) 1.000 0.0290(11)
C4 C Uani 0.4446(7) 0.3575(2) -0.0060(3) 1.000 0.0274(14)
C5 C Uani 0.5466(7) 0.3516(2) 0.1063(3) 1.000 0.0254(12)
C6 C Uani 0.5034(7) 0.4043(2) 0.1738(3) 1.000 0.0206(11)
C7 C Uani 0.6107(6) 0.4031(2) 0.2921(3) 1.000 0.0207(11)
C8 C Uani 0.7459(6) 0.4491(2) 0.4597(3) 1.000 0.0194(11)
C9 C Uani 0.8104(6) 0.3712(2) 0.4686(3) 1.000 0.0191(11)
C10 C Uani 0.9354(7) 0.3194(2) 0.5528(3) 1.000 0.0228(11)
C11 C Uani 0.9658(7) 0.2433(2) 0.5288(3) 1.000 0.0287(14)
C12 C Uani 0.8611(7) 0.2148(2) 0.4192(3) 1.000 0.0276(14)
C13 C Uani 0.7407(7) 0.2624(2) 0.3392(3) 1.000 0.0249(14)
C14 C Uani 0.7792(6) 0.5152(2) 0.5338(3) 1.000 0.0195(11)
C15 C Uani 0.9054(7) 0.5146(2) 0.6466(3) 1.000 0.0237(11)
C16 C Uani 0.9135(7) 0.5836(3) 0.7038(3) 1.000 0.0282(14)
C17 C Uani 0.8032(7) 0.6500(3) 0.6519(3) 1.000 0.0298(14)
C18 C Uani 0.6830(7) 0.6464(2) 0.5402(3) 1.000 0.0275(14)
H2 H Uiso 0.15110 0.50940 -0.02290 1.000 0.0330
H3 H Uiso 0.22550 0.41910 -0.12960 1.000 0.0350
H4 H Uiso 0.47600 0.32130 -0.05070 1.000 0.0320
H5 H Uiso 0.64780 0.31100 0.13820 1.000 0.0300
H10 H Uiso 0.99820 0.33760 0.62610 1.000 0.0270
H11 H Uiso 1.05630 0.20910 0.58470 1.000 0.0340
H12 H Uiso 0.87820 0.16090 0.40360 1.000 0.0330
H13 H Uiso 0.66860 0.24230 0.26740 1.000 0.0300
H15 H Uiso 0.98220 0.46870 0.68220 1.000 0.0280
H16 H Uiso 0.99670 0.58500 0.78020 1.000 0.0340
H17 H Uiso 0.80910 0.69720 0.69140 1.000 0.0360
H18 H Uiso 0.60570 0.69200 0.50360 1.000 0.0330
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V1 0.0234(4) 0.0206(3) 0.0224(3) 0.0031(3) 0.0105(3) 0.0018(3)
O1 0.0252(16) 0.0258(14) 0.0239(14) 0.0003(11) 0.0095(13) 0.0042(14)
O2 0.0260(17) 0.0359(16) 0.0228(14) 0.0020(12) 0.0113(13) -0.0010(15)
O3 0.0290(18) 0.0240(14) 0.0288(14) 0.0026(12) 0.0153(14) 0.0049(14)
N1 0.0208(19) 0.0181(15) 0.0184(15) 0.0013(13) 0.0063(14) 0.0018(15)
N2 0.0175(18) 0.0179(15) 0.0205(16) 0.0001(13) 0.0088(15) 0.0010(14)
N3 0.026(2) 0.0232(16) 0.0237(16) -0.0029(14) 0.0119(15) -0.0024(17)
C1 0.027(2) 0.0208(19) 0.0221(19) -0.0015(15) 0.0151(18) -0.0028(18)
C2 0.024(2) 0.030(2) 0.026(2) 0.0090(17) 0.0092(19) 0.002(2)
C3 0.030(2) 0.034(2) 0.0209(19) -0.0003(18) 0.0089(19) -0.006(2)
C4 0.031(3) 0.029(2) 0.0203(19) -0.0043(17) 0.0092(19) -0.005(2)
C5 0.026(2) 0.023(2) 0.026(2) 0.0007(16) 0.0099(19) 0.0008(19)
C6 0.022(2) 0.0214(19) 0.0181(18) -0.0007(14) 0.0082(17) -0.0029(18)
C7 0.020(2) 0.023(2) 0.0201(18) -0.0005(15) 0.0095(18) 0.0002(17)
C8 0.017(2) 0.0224(18) 0.0179(18) 0.0020(15) 0.0066(16) -0.0016(17)
C9 0.014(2) 0.0242(19) 0.0163(18) 0.0004(15) 0.0037(16) -0.0025(17)
C10 0.019(2) 0.030(2) 0.0190(19) 0.0034(16) 0.0078(17) -0.0007(19)
C11 0.026(3) 0.027(2) 0.031(2) 0.0085(18) 0.010(2) 0.003(2)
C12 0.030(3) 0.0213(19) 0.034(2) 0.0004(17) 0.016(2) 0.000(2)
C13 0.029(3) 0.0184(19) 0.027(2) -0.0059(16) 0.0116(19) -0.0033(19)
C14 0.015(2) 0.0217(19) 0.0237(19) 0.0003(15) 0.0102(17) -0.0001(17)
C15 0.025(2) 0.029(2) 0.0182(19) 0.0030(16) 0.0102(18) -0.0045(19)
C16 0.029(3) 0.036(2) 0.024(2) -0.0040(19) 0.0154(19) -0.011(2)
C17 0.037(3) 0.025(2) 0.037(2) -0.0092(18) 0.025(2) -0.008(2)
C18 0.029(3) 0.024(2) 0.030(2) 0.0007(17) 0.013(2) 0.002(2)
#===============================================================================
# 10. MOLECULAR GEOMETRY
_geom_special_details
;
Bond distances, angles etc. have been calculated using the
rounded fractional coordinates. All esds are estimated
from the variances of the (full) variance-covariance matrix.
The cell esds are taken into account in the estimation of
distances, angles and torsion angles
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.888(3) . . yes
V1 O2 1.610(4) . . yes
V1 O3 1.632(4) . . yes
V1 N1 2.090(3) . . yes
V1 N3 2.173(3) . . yes
O1 C1 1.336(5) . . yes
N1 C7 1.328(5) . . yes
N1 C8 1.368(5) . . yes
N2 C7 1.381(5) . . yes
N2 C9 1.413(4) . . yes
N2 C13 1.393(5) . . yes
N3 C14 1.355(5) . . yes
N3 C18 1.334(5) . . yes
C1 C2 1.411(5) . . no
C1 C6 1.410(6) . . no
C2 C3 1.371(7) . . no
C3 C4 1.374(6) . . no
C4 C5 1.385(5) . . no
C5 C6 1.399(6) . . no
C6 C7 1.455(5) . . no
C8 C9 1.377(5) . . no
C8 C14 1.450(5) . . no
C9 C10 1.410(5) . . no
C10 C11 1.361(5) . . no
C11 C12 1.433(5) . . no
C12 C13 1.326(5) . . no
C14 C15 1.406(5) . . no
C15 C16 1.385(6) . . no
C16 C17 1.374(7) . . no
C17 C18 1.388(5) . . no
C2 H2 0.9498 . . no
C3 H3 0.9494 . . no
C4 H4 0.9506 . . no
C5 H5 0.9505 . . no
C10 H10 0.9511 . . no
C11 H11 0.9505 . . no
C12 H12 0.9511 . . no
C13 H13 0.9492 . . no
C15 H15 0.9499 . . no
C16 H16 0.9500 . . no
C17 H17 0.9494 . . no
C18 H18 0.9507 . . no
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 O2 106.70(14) . . . yes
O1 V1 O3 99.68(15) . . . yes
O1 V1 N1 81.44(12) . . . yes
O1 V1 N3 148.28(13) . . . yes
O2 V1 O3 109.02(16) . . . yes
O2 V1 N1 110.10(16) . . . yes
O2 V1 N3 99.50(15) . . . yes
O3 V1 N1 138.68(15) . . . yes
O3 V1 N3 88.10(14) . . . yes
N1 V1 N3 72.87(12) . . . yes
V1 O1 C1 129.8(3) . . . yes
V1 N1 C7 129.9(2) . . . yes
V1 N1 C8 120.8(2) . . . yes
C7 N1 C8 109.3(3) . . . yes
C7 N2 C9 108.5(3) . . . yes
C7 N2 C13 130.8(3) . . . yes
C9 N2 C13 120.6(3) . . . yes
V1 N3 C14 119.5(2) . . . yes
V1 N3 C18 121.0(3) . . . yes
C14 N3 C18 119.6(3) . . . yes
O1 C1 C2 117.4(4) . . . yes
O1 C1 C6 123.7(3) . . . yes
C2 C1 C6 118.8(4) . . . no
C1 C2 C3 120.6(4) . . . no
C2 C3 C4 120.8(4) . . . no
C3 C4 C5 119.7(4) . . . no
C4 C5 C6 121.2(4) . . . no
C1 C6 C5 118.6(3) . . . no
C1 C6 C7 117.3(3) . . . no
C5 C6 C7 123.8(4) . . . no
N1 C7 N2 108.0(3) . . . yes
N1 C7 C6 122.6(3) . . . yes
N2 C7 C6 129.3(3) . . . yes
N1 C8 C9 109.5(3) . . . yes
N1 C8 C14 114.4(3) . . . yes
C9 C8 C14 136.1(4) . . . no
N2 C9 C8 104.6(3) . . . yes
N2 C9 C10 118.4(3) . . . yes
C8 C9 C10 136.9(3) . . . no
C9 C10 C11 119.8(3) . . . no
C10 C11 C12 119.9(3) . . . no
C11 C12 C13 121.0(3) . . . no
N2 C13 C12 119.9(3) . . . yes
N3 C14 C8 112.4(3) . . . yes
N3 C14 C15 121.5(3) . . . yes
C8 C14 C15 126.1(3) . . . no
C14 C15 C16 117.4(3) . . . no
C15 C16 C17 121.1(4) . . . no
C16 C17 C18 118.3(4) . . . no
N3 C18 C17 122.1(4) . . . yes
C1 C2 H2 119.71 . . . no
C3 C2 H2 119.69 . . . no
C2 C3 H3 119.53 . . . no
C4 C3 H3 119.63 . . . no
C3 C4 H4 120.11 . . . no
C5 C4 H4 120.17 . . . no
C4 C5 H5 119.44 . . . no
C6 C5 H5 119.34 . . . no
C9 C10 H10 120.07 . . . no
C11 C10 H10 120.16 . . . no
C10 C11 H11 120.03 . . . no
C12 C11 H11 120.04 . . . no
C11 C12 H12 119.47 . . . no
C13 C12 H12 119.50 . . . no
N2 C13 H13 119.98 . . . no
C12 C13 H13 120.15 . . . no
C14 C15 H15 121.35 . . . no
C16 C15 H15 121.27 . . . no
C15 C16 H16 119.42 . . . no
C17 C16 H16 119.49 . . . no
C16 C17 H17 120.84 . . . no
C18 C17 H17 120.82 . . . no
N3 C18 H18 118.91 . . . no
C17 C18 H18 118.95 . . . no
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 V1 O1 C1 66.0(3) . . . . no
O3 V1 O1 C1 179.4(3) . . . . no
N1 V1 O1 C1 -42.5(3) . . . . no
N3 V1 O1 C1 -78.4(5) . . . . no
O1 V1 N1 C7 18.2(4) . . . . no
O1 V1 N1 C8 -159.2(3) . . . . no
O2 V1 N1 C7 -86.6(4) . . . . no
O2 V1 N1 C8 96.1(3) . . . . no
O3 V1 N1 C7 113.1(4) . . . . no
O3 V1 N1 C8 -64.3(4) . . . . no
N3 V1 N1 C7 179.4(4) . . . . no
N3 V1 N1 C8 2.0(3) . . . . no
O1 V1 N3 C14 37.8(5) . . . . no
O1 V1 N3 C18 -143.1(4) . . . . no
O2 V1 N3 C14 -107.8(4) . . . . no
O2 V1 N3 C18 71.3(4) . . . . no
O3 V1 N3 C14 143.3(4) . . . . no
O3 V1 N3 C18 -37.7(4) . . . . no
N1 V1 N3 C14 0.5(3) . . . . no
N1 V1 N3 C18 179.5(4) . . . . no
V1 O1 C1 C2 -139.2(4) . . . . no
V1 O1 C1 C6 43.4(6) . . . . no
V1 N1 C7 N2 -176.7(3) . . . . no
V1 N1 C7 C6 6.2(7) . . . . no
C8 N1 C7 N2 0.9(5) . . . . no
C8 N1 C7 C6 -176.2(4) . . . . no
V1 N1 C8 C9 177.8(3) . . . . no
V1 N1 C8 C14 -4.0(5) . . . . no
C7 N1 C8 C9 0.0(5) . . . . no
C7 N1 C8 C14 178.2(4) . . . . no
C9 N2 C7 N1 -1.4(5) . . . . no
C9 N2 C7 C6 175.4(5) . . . . no
C13 N2 C7 N1 175.0(4) . . . . no
C13 N2 C7 C6 -8.2(8) . . . . no
C7 N2 C9 C8 1.3(5) . . . . no
C7 N2 C9 C10 -178.2(4) . . . . no
C13 N2 C9 C8 -175.5(4) . . . . no
C13 N2 C9 C10 5.0(6) . . . . no
C7 N2 C13 C12 178.0(5) . . . . no
C9 N2 C13 C12 -5.9(7) . . . . no
V1 N3 C14 C8 -2.5(5) . . . . no
V1 N3 C14 C15 177.6(3) . . . . no
C18 N3 C14 C8 178.4(4) . . . . no
C18 N3 C14 C15 -1.5(7) . . . . no
V1 N3 C18 C17 -178.1(4) . . . . no
C14 N3 C18 C17 1.0(7) . . . . no
O1 C1 C2 C3 178.6(5) . . . . no
C6 C1 C2 C3 -3.8(7) . . . . no
C2 C1 C6 C7 179.9(3) . . . . no
C2 C1 C6 C5 5.1(7) . . . . no
O1 C1 C6 C5 -177.5(4) . . . . no
O1 C1 C6 C7 -2.7(7) . . . . no
C1 C2 C3 C4 0.5(8) . . . . no
C2 C3 C4 C5 1.5(7) . . . . no
C3 C4 C5 C6 -0.2(7) . . . . no
C4 C5 C6 C1 -3.1(7) . . . . no
C4 C5 C6 C7 -177.6(4) . . . . no
C1 C6 C7 N1 -19.4(7) . . . . no
C1 C6 C7 N2 164.3(4) . . . . no
C5 C6 C7 N1 155.1(4) . . . . no
C5 C6 C7 N2 -21.2(8) . . . . no
N1 C8 C9 C10 178.6(5) . . . . no
C14 C8 C9 N2 -178.5(5) . . . . no
N1 C8 C9 N2 -0.8(5) . . . . no
C9 C8 C14 C15 1.4(9) . . . . no
C14 C8 C9 C10 0.9(10) . . . . no
N1 C8 C14 N3 4.0(6) . . . . no
N1 C8 C14 C15 -176.2(4) . . . . no
C9 C8 C14 N3 -178.4(5) . . . . no
C8 C9 C10 C11 -179.5(5) . . . . no
N2 C9 C10 C11 -0.2(7) . . . . no
C9 C10 C11 C12 -3.6(7) . . . . no
C10 C11 C12 C13 2.8(8) . . . . no
C11 C12 C13 N2 2.1(8) . . . . no
N3 C14 C15 C16 1.1(7) . . . . no
C8 C14 C15 C16 -178.7(5) . . . . no
C14 C15 C16 C17 -0.4(8) . . . . no
C15 C16 C17 C18 -0.1(8) . . . . no
C16 C17 C18 N3 -0.2(8) . . . . no
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
V1 C12 3.785(4) . 2_655 no
V1 C13 3.657(4) . 2_655 no
V1 C15 3.495(5) . 3_666 no
V1 C16 3.914(5) . 3_666 no
V1 C14 3.785(4) . 3_666 no
V1 H12 3.2427 . 2_655 no
V1 H13 2.9778 . 2_655 no
V1 H15 3.5010 . 3_666 no
O1 C15 3.357(6) . 3_666 no
O1 C16 3.204(6) . 3_666 no
O2 C10 3.061(6) . 3_766 no
O2 C13 3.246(5) . 2_655 no
O2 C3 3.310(5) . 3_665 no
O2 C4 3.399(5) . 3_665 no
O3 C15 3.072(5) . 3_666 no
O3 C10 3.021(6) . 3_666 no
O3 C14 3.409(5) . 3_666 no
O3 C9 3.300(5) . 3_666 no
O3 C13 2.994(5) . 2_655 no
O3 C12 3.285(5) . 2_655 no
O1 H12 2.7052 . 2_655 no
O2 H3 2.6650 . 3_665 no
O2 H10 2.4130 . 3_766 no
O2 H4 2.8483 . 3_665 no
O2 H13 2.6856 . 2_655 no
O3 H13 2.2299 . 2_655 no
O3 H12 2.8327 . 2_655 no
O3 H18 2.6116 . . no
O3 H10 2.6333 . 3_666 no
O3 H15 2.7077 . 3_666 no
N1 C15 3.329(7) . 3_766 no
N2 C16 3.316(6) . 3_766 no
N3 C10 3.447(6) . 3_766 no
N3 C8 3.409(6) . 3_666 no
N2 H5 2.8878 . . no
C1 C3 3.574(7) . 3_665 no
C2 C3 3.545(7) . 3_665 no
C3 C2 3.545(7) . 3_665 no
C3 O2 3.310(5) . 3_665 no
C3 C1 3.574(7) . 3_665 no
C4 O2 3.399(5) . 3_665 no
C5 C13 3.230(5) . . no
C7 C15 3.452(7) . 3_766 no
C7 C16 3.352(7) . 3_766 no
C7 C17 3.444(7) . 3_666 no
C8 N3 3.409(6) . 3_666 no
C8 C15 3.403(7) . 3_766 no
C8 C14 3.379(7) . 3_766 no
C8 C18 3.436(7) . 3_666 no
C9 C18 3.456(7) . 3_666 no
C9 C14 3.490(6) . 3_766 no
C9 O3 3.300(5) . 3_666 no
C9 C15 3.587(6) . 3_766 no
C10 O3 3.021(6) . 3_666 no
C10 O2 3.061(6) . 3_766 no
C10 C15 3.563(5) . . no
C10 C18 3.482(7) . 3_766 no
C10 N3 3.447(6) . 3_766 no
C11 C18 3.534(7) . 3_766 no
C12 O3 3.285(5) . 2_645 no
C12 V1 3.785(4) . 2_645 no
C13 C5 3.230(5) . . no
C13 O2 3.246(5) . 2_645 no
C13 C17 3.504(7) . 3_766 no
C13 O3 2.994(5) . 2_645 no
C13 V1 3.657(4) . 2_645 no
C14 C8 3.379(7) . 3_766 no
C14 V1 3.785(4) . 3_666 no
C14 O3 3.409(5) . 3_666 no
C14 C9 3.490(6) . 3_766 no
C15 C7 3.452(7) . 3_766 no
C15 O1 3.357(6) . 3_666 no
C15 O3 3.072(5) . 3_666 no
C15 C9 3.587(6) . 3_766 no
C15 N1 3.329(7) . 3_766 no
C15 V1 3.495(5) . 3_666 no
C15 C8 3.403(7) . 3_766 no
C15 C10 3.563(5) . . no
C16 N2 3.316(6) . 3_766 no
C16 O1 3.204(6) . 3_666 no
C16 C7 3.352(7) . 3_766 no
C16 V1 3.914(5) . 3_666 no
C17 C7 3.444(7) . 3_666 no
C17 C13 3.504(7) . 3_766 no
C18 C9 3.456(7) . 3_666 no
C18 C8 3.436(7) . 3_666 no
C18 C11 3.534(7) . 3_766 no
C18 C10 3.482(7) . 3_766 no
C2 H2 2.9629 . 3_565 no
C3 H12 3.0560 . 4_454 no
C4 H18 2.8105 . 2_645 no
C5 H18 3.0389 . 2_645 no
C5 H13 2.7025 . . no
C6 H13 3.0253 . . no
C9 H15 3.0942 . . no
C10 H15 3.0025 . . no
C12 H4 2.9860 . 4_555 no
C13 H5 2.6488 . . no
C15 H10 3.0890 . . no
H2 C2 2.9629 . 3_565 no
H2 H2 2.4891 . 3_565 no
H3 H15 2.5378 . 1_454 no
H3 O2 2.6650 . 3_665 no
H4 H18 2.4073 . 2_645 no
H4 O2 2.8483 . 3_665 no
H4 C12 2.9860 . 4_554 no
H5 N2 2.8878 . . no
H5 C13 2.6488 . . no
H5 H13 2.0529 . . no
H10 C15 3.0890 . . no
H10 H15 2.3529 . . no
H10 O2 2.4130 . 3_766 no
H10 O3 2.6333 . 3_666 no
H12 V1 3.2427 . 2_645 no
H12 O1 2.7052 . 2_645 no
H12 O3 2.8327 . 2_645 no
H12 C3 3.0560 . 4_655 no
H13 C5 2.7025 . . no
H13 C6 3.0253 . . no
H13 H5 2.0529 . . no
H13 V1 2.9778 . 2_645 no
H13 O2 2.6856 . 2_645 no
H13 O3 2.2299 . 2_645 no
H15 C9 3.0942 . . no
H15 C10 3.0025 . . no
H15 H3 2.5378 . 1_656 no
H15 H10 2.3529 . . no
H15 V1 3.5010 . 3_666 no
H15 O3 2.7077 . 3_666 no
H18 O3 2.6116 . . no
H18 C4 2.8105 . 2_655 no
H18 C5 3.0389 . 2_655 no
H18 H4 2.4073 . 2_655 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
#
#D H A D - H H...A D...A D - H...A symm(A)
#
C10 H10 O2 0.9511 2.4130 3.061(6) 125.14 3_766 yes
C13 H13 O3 0.9492 2.2299 2.994(5) 136.92 2_645 yes
# End of Crystallographic Information File
#===========================================================================
# Dr. A.L.Spek, Laboratory of Crystal and Structural Chemistry #
# Bijvoet Center for Biomolecular Research, Utrecht University. #
# (Kruytgebouw, room N801), Padualaan 8, 3584 CH Utrecht, The Netherlands. #
# E-mail: a.l.spek@chem.uu.nl http://www.cryst.chem.uu.nl/ #
# http://www.cryst.chem.uu.nl/platon/ #
# anonymous ftp: xraysoft.chem.uu.nl #
# FAX : (31)-30-2533940 PHONE : (31)-30-2532538/2533/3902/3502 #
#===========================================================================